CN104987516B - A kind of nano-cellulose strengthens the preparation method of tara gum substrate pH intelligent response film - Google Patents
A kind of nano-cellulose strengthens the preparation method of tara gum substrate pH intelligent response film Download PDFInfo
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Abstract
A kind of nano-cellulose strengthens the preparation method of tara gum substrate pH intelligent response film, and it is related to the preparation method of pH intelligent response films.Complicated, the high cost technical problem the present invention is to solve existing pH responsive materials preparation technology.This method：Microcrystalline cellulose is made nano-cellulose through dense sulfuric acid treatment；Grape skin extract is prepared, glycerine, nano-cellulose and grape skin extract are added into tara gum solution, after stirring, obtain into film liquid；Casting film-forming, drying, obtain nano-cellulose enhancing tara gum substrate pH intelligent response film.The film color can change in acid or alkali environment, can be used to make packaging material.
Description
Technical field
The present invention relates to the preparation method of pH intelligent response films.
Background technology
In recent years, people propose new demand to the packaging of food, it is desirable to which packaging material are more and more safer, reduce addition
The addition of agent, while wishing that packaging material are more and more intelligent again, can monitor the fresh-keeping spoilage problem of food or medicine.Such as
The Chinese patent of Application No. 201310370689.2 discloses a kind of Biodegradable polymer vesicles of pH responses, the material
It is the triblock polymer of poly glycol monomethyl ether, poly- (6-caprolactone) and polyglutamic acid, is mainly used in carrying medicine, it passes through to add
Various initiators realize pH responses and carry medicine effect, preparation technology complexity, high cost.
The content of the invention
Complicated, the high cost technical problem the present invention is to solve existing pH responsive materials preparation technology, and provide a kind of
Nano-cellulose strengthens the preparation method of tara gum substrate pH intelligent response film.
Nano-cellulose of the present invention strengthens the preparation method of tara gum substrate pH intelligent response film, carries out according to the following steps：
First, microcrystalline cellulose (MCC) and concentrated sulfuric acid solution are added to vessel in heating to 45~55 DEG C, reaction 1.5~
3h, obtains cellulose suspension；Wherein the mass concentration of concentrated sulfuric acid solution is 50%~60%；
2nd, after cellulose suspension is washed, the colloidal material of centrifugation bottom of the tube is collected in centrifugation, then is put
In the bag filter that a molecular cut off is 6000~8000, with deionized water as dialyzate, the pH value of dialysis to colloid is
Neutrality, then 15~30min is processed with ultrasonic cell disruptor, dry, obtain nano-cellulose；
3rd, Grape Skin is cleaned and is crushed after drying, be 1 by grape skin powder and leaching liquor mass ratio：(1.5~2.5), by Portugal
Grape skin powder is added in leaching liquor, then adjusts pH value to 1~2；12~24h is extracted under the conditions of 0~10 DEG C, is then in temperature
Rotary evaporation under conditions of 30~40 DEG C, after re-dry to constant weight, obtains grape skin extract；
4th, after tara gum is crushed, tara gum is added to the water for 0.5~2% by the mass percentage concentration of tara gum, plus
Heat stirs 2~5h to 40~50 DEG C, is then centrifuged for removing insoluble impurity, obtains tara gum solution；Tower in tara gum solution is pressed again
The 25%~35% of colloid amount is drawn to weigh glycerine, weighing step 2 by 4%~10% of tara gum quality in tara gum solution obtains
The nano-cellulose for arriving, grape skin extract is weighed by 5%~15% of tara gum quality in tara gum solution, by glycerine, is received
Rice cellulose and grape skin extract add tara gum solution, after stirring, obtain into film liquid；
5th, into after film liquid de-bubble, casting film-forming is dried under conditions of being 55~65 DEG C in temperature, obtains nano-cellulose
Enhancing tara gum substrate pH intelligent response film.
The present invention is prepared nano-cellulose, anthocyanidin is extracted using discarded object Grape Skin and is added using microcrystalline cellulose
It is added in tara gum, obtains the pH response smart membranes with good mechanical properties.The present invention has advantages below：The present invention is
With tara gum as main film forming substance, nano-cellulose and grape skin extract are added, preparing, there is pH to respond smart membrane material,
Improve the pliability of thin-film material again simultaneously.Preparing nano-cellulose strengthens the main original of tara gum substrate pH intelligent response film
Material and auxiliary material are edibility material, such as tara gum, and a kind of natural polysaccharide, grape skin extract contains flavonoid substances, has
Good antioxidation activity, it is nontoxic to human body, safety non-toxic is used as packaging material for food, and biological can drop completely
Solution.
The anthocyanidin that the present invention is extracted using natural products Grape Skin, process is simple and realizes the reasonable utilization of resource, system
Standby intelligent response film color can change in acid or alkali environment, can be used to make packaging material.
Brief description of the drawings
The size distribution curve figure of the nano-cellulose in the step of Fig. 1 is embodiment 1 two；
Ultraviolet-visible light of the grape skin extract that the step of Fig. 2 is embodiment 1 three obtains in the different pH value aqueous solution
Abosrption spectrogram；
Fig. 3 is the tara gum of embodiment 1, the amount of filling of nano-cellulose is 0% tara gum substrate pH intelligent response film,
The amount of filling of nano-cellulose is 2%, 4%, 6% and 8% nano-cellulose enhancing tara gum substrate pH intelligent response film
Infrared spectrogram；
Fig. 4 is the tara gum of embodiment 1, the amount of filling of nano-cellulose is 0% tara gum substrate pH intelligent response film,
The amount of filling of nano-cellulose is 2%, 4%, 6% and 8% nano-cellulose enhancing tara gum substrate pH intelligent response film
Tensile strength and elongation at break result figure；
Fig. 5 is the tara gum of embodiment 1, the amount of filling of nano-cellulose is 0% tara gum substrate pH intelligent response film,
The amount of filling of nano-cellulose is 2%, 4%, 6% and 8% nano-cellulose enhancing tara gum substrate pH intelligent response film
Light transmittance curve figure；
Fig. 6 is the infrared spectrogram of nano-cellulose enhancing tara gum substrate pH intelligent response film in embodiment 2.
Specific embodiment
Specific embodiment one：The nano-cellulose of present embodiment strengthens the preparation of tara gum substrate pH intelligent response film
Method, is carried out according to the following steps：
First, microcrystalline cellulose (MCC) and concentrated sulfuric acid solution are added to vessel in heating to 45~55 DEG C, reaction 1.5~
3h, obtains cellulose suspension；Wherein the mass concentration of concentrated sulfuric acid solution is 50%~60%；
2nd, after cellulose suspension is washed, the colloidal material of centrifugation bottom of the tube is collected in centrifugation, then is put
In the bag filter that a molecular cut off is 6000~8000, with deionized water as dialyzate, the pH value of dialysis to colloid is
Neutrality, then 15~30min is processed with ultrasonic cell disruptor, dry, obtain nano-cellulose (NCC)；
3rd, Grape Skin is cleaned and is crushed after drying, be 1 by grape skin powder and leaching liquor mass ratio：(1.5~2.5), by Portugal
Grape skin powder is added in leaching liquor, then adjusts pH value to 1~2；12~24h is extracted under the conditions of 0~10 DEG C, is then in temperature
Rotary evaporation under conditions of 30~40 DEG C, after re-dry to constant weight, obtains grape skin extract；
4th, after tara gum is crushed, tara gum is added to the water for 0.5~2% by the mass percentage concentration of tara gum, plus
Heat stirs 2~5h to 40~50 DEG C, is then centrifuged for removing insoluble impurity, obtains tara gum solution；Tower in tara gum solution is pressed again
The 25%~35% of colloid amount is drawn to weigh glycerine, weighing step 2 by 4%~10% of tara gum quality in tara gum solution obtains
The nano-cellulose for arriving, grape skin extract is weighed by glycerine, nanometer by 5%~15% of tara gum quality in tara gum solution
Cellulose and grape skin extract add tara gum solution, after stirring, obtain into film liquid；
5th, into after film liquid de-bubble, casting film-forming is dried under conditions of being 55~65 DEG C in temperature, obtains nano-cellulose
Enhancing tara gum substrate pH intelligent response film.
Specific embodiment two：Present embodiment from step one unlike specific embodiment one heat temperature be
51 DEG C, the reaction time is 2.5h.Other are identical with specific embodiment one.
Specific embodiment three：Present embodiment is molten from the concentrated sulfuric acid in step one unlike specific embodiment one or two
The mass concentration of liquid is 56%.Other are identical with specific embodiment one or two.
Specific embodiment four：Ultrasound in step 2 unlike one of present embodiment and specific embodiment one to three
Ripple cell disruptor process time is 20min.Other are identical with one of specific embodiment one to three.
Specific embodiment five：Extracted in step 3 unlike one of present embodiment and specific embodiment one to four
Liquid is ethanol, propyl alcohol, isopropanol or water.Other are identical with one of specific embodiment one to four.
Specific embodiment six：Nanometer in step 4 unlike one of present embodiment and specific embodiment one to five
The quality of cellulose is 8% of tara gum quality in tara gum solution, and the quality of grape skin extract is tower in tara gum solution
Draw the 5%-15% of colloid amount.Other are identical with one of specific embodiment one to five.
Specific embodiment seven：Dried in step 5 unlike one of present embodiment and specific embodiment one to six
Temperature is 60 DEG C.Other are identical with one of specific embodiment one to six.
With following verification experimental verification beneficial effects of the present invention：
Embodiment 1：
The nano-cellulose of the present embodiment strengthens the preparation method of tara gum substrate pH intelligent response film, enters according to the following steps
OK：
First, microcrystalline cellulose (MCC) and concentrated sulfuric acid solution are added to vessel in heating to 50 DEG C, react 2h, obtain fibre
The plain suspension of dimension；Wherein the mass concentration of concentrated sulfuric acid solution is 55%；
2nd, after cellulose suspension is washed, the colloidal material of centrifugation bottom of the tube is collected in centrifugation, then is put
In the bag filter that a molecular cut off is 7000, with deionized water as dialyzate, the pH value of dialysis to colloid is 7, then is used
Ultrasonic cell disruptor processes 20min, dries, and obtains nano-cellulose；
3rd, Grape Skin is cleaned and is crushed after drying, be 1 by grape skin powder and ethanol mass ratio：2, grape skin powder is added
In ethanol, pH value to 2.0 is then adjusted；It is placed in 5 DEG C of refrigerator and extracts 12h, is rotated under conditions of being then 40 DEG C in temperature
Evaporating ethanol, dries to constant weight, obtains grape skin extract；
4th, after tara gum is crushed, tara gum is added to the water for 0.75% by the mass percentage concentration of tara gum, is heated
To 45 DEG C, 3h is stirred, be then centrifuged for removing insoluble impurity, obtain tara gum solution；Tara gum quality in tara gum solution is pressed again
30% weigh glycerine, weighing step 2 respectively by 0%, 2%, 4%, 6% and 8% of tara gum quality in tara gum solution obtains
The nano-cellulose for arriving, then grape skin extract is weighed by 6% of tara gum quality in tara gum solution, by glycerine, Nanowire
Dimension element and grape skin extract add tara gum solution, after stirring, obtain into film liquid；
5th, into after film liquid de-bubble, casting film-forming is dried under conditions of being 60 DEG C in temperature, obtains nano-cellulose enhancing
Tara gum substrate pH intelligent response film.
The yield of the nano-cellulose obtained in the present embodiment step 2 is 69.50%.The granularity of the nano-cellulose point
Cloth curve is as shown in figure 1, from figure 1 it appears that the granularity of nano-cellulose is mainly distributed on 151nm, having and being distributed on a small quantity
4nm.The PDI values of granulometry experiment are 1.00, illustrate that yardstick difference is smaller, and the nano-cellulose of preparation is than more uniform.
Uv-visible absorption spectroscopy of the grape skin extract that step 3 is obtained in the different pH value aqueous solution is as schemed
Shown in 2, figure it is seen that grape skin extract solution has absorption maximum when pH value is 1.0~3.0 near 520nm
Peak, with the increase of pH value, it is seen that the light absorption value at light area maximum absorption band is gradually reduced, finally when anthocyanin solution ph is big
When 4.0, it is seen that the absworption peak in light area disappears.Therefore when pH value changes, the color of grape skin extract can produce change.
By the pure tara gum of the present embodiment, (amount of filling of nano-cellulose is 0% tara gum substrate pH intelligent response
Film), nano-cellulose (NCC) that the amount of filling of nano-cellulose is 2%, 4%, 6% and 8% enhancing tara gum substrate pH intelligence
Response film carries out the test of infrared spectrogram, the infrared spectrogram for obtaining as shown in figure 3, tara gum and not as can be seen from Figure 3
In infrared spectrum with addition nano-cellulose, 3332cm-1Place is the characteristic peak that stronger-OH absorbs, 2933cm-1Locate for-
CH2Stretching vibration peak, 1631cm-1And 1376cm-1Locate to be-OH flexural vibrations absworption peaks, 1007cm-1And 868cm-1It is sugared ring to locate
On C-OH flexural vibrations peak.It can be seen that with the increase of nano-cellulose addition, the absworption peak enhancing explanation of-OH is received
Rice cellulose draws polysaccharide to form intermolecular hydrogen bonding with tower.
Amount of filling by the nano-cellulose of the present embodiment is 0% tara gum substrate pH intelligent response film, nanofiber
The amount of filling of element is that to carry out tension strong for 2%, 4%, 6% and 8% nano-cellulose enhancing tara gum substrate pH intelligent response film
The test of degree and elongation at break, the tensile strength for obtaining and elongation at break result as shown in figure 4, as seen from Figure 4, with
The increase of NCC additions, the tensile strength and elongation at break of composite membrane first increase reduction.This is because NCC and tower draw
Between form hydrogen bond, NCC plays incorgruous nucleation in the polymer, improves the crystal property of polymer, with XRD result phases
Together, so as to improve intensity and elongation at break.But as NCC additions further increase, NCC easily reunites, and limits
Tower draws the movement of matrix, so that elongation at break reduction.Nano-cellulose optimum addition is 6%.
Amount of filling by the nano-cellulose of the present embodiment is 0% tara gum substrate pH intelligent response film, nanofiber
Element amount of filling be 2%, 4%, 6% and 8% nano-cellulose enhancing tara gum substrate pH intelligent response film carry out light transmittance
The test of curve, the light transmittance curve figure for obtaining from Fig. 5 as shown in figure 5, can see with the increase tower of nanofiber cellulose content
Draw polysaccharide composite film printing opacity to reduce after taking the lead in increasing, maximum is reached when nanofiber cellulose content is 6%.The increase of light transmittance
On the one hand explanation nano particle is smaller, and the influence of light scattering is eliminated in visible-range, reaches good light transmittance.It is another
Aspect explanation tower drawing between divide between polysaccharide and nano-cellulose and is tightly combined.When nano-cellulose addition is excessive, due to
The influence of " nano effect " causes light transmittance to reduce but change smaller.
Amount of filling by the nano-cellulose of the present embodiment is 6% nano-cellulose enhancing tara gum substrate pH intelligence sound
Answer film to be placed in pH solution, observe film color change, result is：Color can occur obvious change under different pH, especially
It is that under strongly acidic conditions, color change is still most obvious.Illustrate that the anthocyanidin in composite membrane does not occur chemical change,
Remain in that the chemical property of oneself uniqueness.
Amount of filling by the nano-cellulose of the present embodiment is 6% nano-cellulose enhancing tara gum substrate pH intelligence sound
Film is answered to be placed in Yoghourt, when Yoghourt is rotten causes acid enhancing, film color is changed into pale red from inclined yellow, can warn Yoghourt
Mass change.
Food, in putrid and deteriorated process, is the flourish process of microorganism, can produce some acid in this process
Material, can make the pH of food change, therefore pH respective changes can make people find putrid and deteriorated food in time, improve
Food security.Using membrane material of the invention as packing material, color change can be produced, indicate the deterioration of food.This hair
Bright membrane material can be used as packaging material.
Embodiment 2
The operation of the present embodiment step 4 as different from Example 1 is substituted for：After tara gum is crushed, by tara gum
Be added to the water for tara gum for 0.75% by mass percentage concentration, is heated to 45 DEG C, stirs 3h, is then centrifuged for removing insoluble impurity,
Obtain tara gum solution；Glycerine is weighed by 30% of tara gum quality in tara gum solution again, by tara gum in tara gum solution
The 6% of quality weighs the nano-cellulose that step 2 is obtained, then by 0% of tara gum quality in tara gum solution, 10%, 15%
Grape skin extract is weighed respectively, glycerine, nano-cellulose and grape skin extract are added into tara gum solution, stir
Afterwards, film liquid is obtained into；Other steps are same as Example 1 with parameter.
Nano-cellulose manufactured in the present embodiment strengthens infrared spectrogram such as Fig. 6 institutes of tara gum substrate pH intelligent response film
Show, wherein, a is the infrared spectrogram of the film that grape skin extract addition is 0%, and b is for grape skin extract addition
The infrared spectrogram of 10% film, c is the infrared spectrogram of the film that grape skin extract addition is 15%.Can from Fig. 6
Go out 3418cm-1(- OH stretching vibrations)；2925cm-1(-CH2Stretching vibration)；1645cm-1(H-O-H)；1363cm-1(CH
bending)；1248cm-1(acetate C-O bending)；The stretching vibration absworption peak of 1092cm-1 (- C-O)).
1600cm-1The absworption peak C=C absworption peaks (presence of phenol) for going out, and as the increase absworption peak of anthocyanidin addition is sharpened,
Illustrate in composite membrane with the presence of anthocyanins material.
By the nano-cellulose enhancing tara gum matrix membrane of the present embodiment, (addition of grape skin extract is 0%
Film), (addition of grape skin extract is tara gum quality to nano-cellulose enhancing tara gum substrate pH intelligent response film
10%th, 15% film) it is individually placed in Yoghourt, when Yoghourt is rotten causes acid enhancing, film color is changed into light red from inclined yellow
Color, can warn the mass change of Yoghourt, and nano-cellulose enhancing tara gum matrix membrane is unchanged.Therefore nano-cellulose increases
Strong tara gum substrate pH intelligent response film can reflect the acidity change of the material packaged by it.
By nano-cellulose manufactured in the present embodiment enhancing tara gum matrix membrane, (addition of grape skin extract is 0%
Film), (addition of grape skin extract is 10%, 15% to nano-cellulose enhancing tara gum substrate pH intelligent response film
Film) test of intensity and elongation at break is carried out, its result is as shown in table 1 below：
Influence of the grape skin extract addition of table 1 to intensity and elongation at break
| Grape skin extract addition (%) | Intensity (MPa) | Elongation at break (%) |
| 0 | 65.73 | 3.3 |
| 10 | 50.44 | 49.4 |
| 15 | 40.27 | 54.8 |
As it can be seen from table 1 influence of the addition of grape skin extract to film elongation at break is larger, 10% grape is added
Compared with being not added with, elongation at break improves 46 percentage points to bark extract, adds 15% anthocyanidin, elongation at break rate
51 percentage points are improved, illustrates that grape skin extract in addition to being acted on pH responses, also increases the flexible effect of film.
Claims (7)
1. a kind of nano-cellulose strengthens the preparation method of tara gum substrate pH intelligent response film, it is characterised in that the method press with
Lower step is carried out：
First, microcrystalline cellulose and concentrated sulfuric acid solution are added to vessel in heating to 45~55 DEG C, react 1.5~3h, obtain fibre
The plain suspension of dimension；Wherein the mass concentration of concentrated sulfuric acid solution is 50%~60%；
2nd, after cellulose suspension is washed, the colloidal material of centrifugation bottom of the tube is collected in centrifugation, then by colloidal thing
Matter is placed in the bag filter that a molecular cut off is 6000~8000, with deionized water as dialyzate, the pH of dialysis to colloid
It is neutrality to be worth, then processes 15~30min with ultrasonic cell disruptor, is dried, and obtains nano-cellulose；
3rd, Grape Skin is cleaned and is crushed after drying, be 1 by grape skin powder and leaching liquor mass ratio：(1.5~2.5), by Grape Skin
Powder is added in leaching liquor, then adjusts pH value to 1~2；Under the conditions of 0~10 DEG C extract 12~24h, then temperature be 30~
Rotary evaporation under conditions of 40 DEG C, after re-dry to constant weight, obtains grape skin extract；
4th, after tara gum is crushed, tara gum is added to the water for 0.5~2% by the mass percentage concentration of tara gum, is heated to
40~50 DEG C, 2~5h is stirred, be then centrifuged for removing insoluble impurity, obtain tara gum solution；Tara gum in tara gum solution is pressed again
The 25%~35% of quality weighs glycerine, weighs what step 2 was obtained by 4%~10% of tara gum quality in tara gum solution
Nano-cellulose, grape skin extract is weighed by 5%~15% of tara gum quality in tara gum solution, by glycerine, Nanowire
Dimension element and grape skin extract add tara gum solution, after stirring, obtain into film liquid；
5th, into after film liquid de-bubble, casting film-forming is dried under conditions of being 55~65 DEG C in temperature, obtains nano-cellulose enhancing
Tara gum substrate pH intelligent response film.
2. a kind of nano-cellulose according to claim 1 strengthens the preparation method of tara gum substrate pH intelligent response film,
It is characterized in that the temperature heated in step one is 51 DEG C, the reaction time is 2.5h.
3. a kind of nano-cellulose according to claim 1 and 2 strengthens the preparation side of tara gum substrate pH intelligent response film
Method, it is characterised in that the mass concentration of concentrated sulfuric acid solution is 56% in step one.
4. a kind of nano-cellulose according to claim 1 and 2 strengthens the preparation side of tara gum substrate pH intelligent response film
Method, it is characterised in that the power of ultrasonic cell disruptor is 1000W in step 2, and process time is 20min.
5. a kind of nano-cellulose according to claim 1 and 2 strengthens the preparation side of tara gum substrate pH intelligent response film
Method, it is characterised in that leaching liquor is ethanol, propyl alcohol, isopropanol or water in step 3.
6. a kind of nano-cellulose according to claim 1 and 2 strengthens the preparation side of tara gum substrate pH intelligent response film
Method, it is characterised in that the quality of nano-cellulose is 8% of tara gum quality in tara gum solution in step 4, and Grape Skin is extracted
The quality of thing is 12% of tara gum quality in tara gum solution.
7. a kind of nano-cellulose according to claim 1 and 2 strengthens the preparation side of tara gum substrate pH intelligent response film
Method, it is characterised in that drying temperature is 60 DEG C in step 5.
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| CN106117577B (en) * | 2016-08-01 | 2019-02-19 | 东北林业大学 | A kind of curcumin/PVA/ tara gum NH3The preparation method of intelligent response film |
| CN107057127A (en) * | 2017-05-02 | 2017-08-18 | 上海海洋大学 | A kind of preparation method of pH responsive nanos cellulose antibacterial controlled release membranes |
| CN107602941B (en) * | 2017-09-04 | 2021-01-05 | 北京林业大学 | PH-sensitive gleditsia sinensis polysaccharide composite membrane and preparation method thereof |
| CN108314792B (en) * | 2018-02-08 | 2020-07-28 | 东北林业大学 | Preparation method of pH intelligent response membrane capable of firmly locking anthocyanidin |
| CN108586825A (en) * | 2018-04-24 | 2018-09-28 | 黄正农 | A kind of fast sample material of food spoilage with pH discoloration responses and preparation method thereof, purposes |
| CN109030482A (en) * | 2018-10-30 | 2018-12-18 | 顺德职业技术学院 | A kind of intelligence suction pipe |
| CN109797584B (en) * | 2019-02-27 | 2021-08-13 | 青岛威达体育用品有限公司 | Variable-color intelligent induction fabric prepared by inkless jet printing technology and preparation method thereof |
| CN113229362B (en) * | 2021-05-10 | 2022-08-26 | 东北林业大学 | Preparation method of polyanion anti-shrinkage fruit fresh-keeping coating liquid |
| CN114316320A (en) * | 2022-01-25 | 2022-04-12 | 集美大学 | Degradable pH-responsive intelligent packaging material and preparation method thereof |
| CN115353568B (en) * | 2022-08-16 | 2024-02-06 | 河北农业大学 | Carboxylated cellulose nanocrystalline, intelligent film, preparation method and application |
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